CN106891273A - A kind of novel nano vitrified bond and its preparation method and application - Google Patents

Abstract

The invention discloses a novel nano-ceramic bonding agent and a preparation method thereof, belonging to the field of nano-composite materials and mechanical processing. The specific method includes the following steps: preparing a titanate one-dimensional nanomaterial; providing Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic ceramic bond powder; The addition amount of ~5wt% is added to the basic vitrified bond powder, fully mixed and dispersed evenly, and the nano vitrified bond is prepared. Because the existing ordinary vitrified bond has the disadvantages of low strength, high sintering temperature and its own brittleness, the nano-ceramic bond prepared by adding a titanate one-dimensional nanomaterial in the present invention overcomes the shortcomings of the ordinary vitrified bond. Not only greatly reduces the sintering temperature of the bonding agent, saves energy, but also significantly improves the strength of the vitrified bonding agent, and is well applied to ceramic grinding tools.

Description

A novel nano-ceramic bond and its preparation method and application

technical field

The invention belongs to the field of nano-composite materials and mechanical processing, in particular to a novel nano-ceramic bonding agent and its preparation method and application.

Background technique

With the development of the modern precision machining industry, the requirements for processing tools are getting higher and higher, and the importance of ceramic abrasive tools is becoming increasingly apparent. However, there are still some problems in the high-end precision grinding of ceramic abrasive tools. The existing ordinary vitrified bond It has the disadvantages of low strength, high sintering temperature and its own brittleness, which cannot meet the processing strength requirements of ceramic abrasive tools, which requires us to further improve the vitrified bond. Therefore, it is necessary to explore a vitrified bond with low sintering temperature and high strength, which can well meet the needs of ceramic abrasive tools in precision machining.

Contents of the invention

In order to solve the problems existing in the prior art, the invention provides a kind of preparation method of novel nano vitrified bond, comprising the following steps:

S1: Preparation of titanate one-dimensional nanomaterials;

S2: Provide Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic vitrified bond powder;

S3: Add the titanate one-dimensional nanomaterial prepared in S1 to the basic vitrified bond powder in an amount of 0.2-5wt%, fully mix and disperse evenly, and prepare a nano vitrified bond.

Preferably, the raw material used to prepare the titanate one-dimensional nanomaterial is titanium dioxide, metal titanium, titanium alloy or titanium salt.

More preferably, the titanate one-dimensional nanomaterial is sodium titanate nanowire, potassium titanate nanowire, sodium titanate nanofiber, potassium titanate nanofiber, sodium titanate nanobelt, potassium titanate nanobelt any of the

More preferably, the specific steps of S1 are: preparing a 10mol/L sodium hydroxide or potassium hydroxide solution for subsequent use;

Weigh the titanium dioxide powder, add the titanium dioxide powder into the sodium hydroxide or potassium hydroxide solution according to the solid-to-liquid ratio of 1g: 20-40ml, fully dissolve to obtain a mixed solution;

The mixed solution is added into a hydrothermal reaction kettle, kept at 140-160°C for 8-10h, then naturally cooled to room temperature, washed, centrifuged and dried, then calcined at 420-450°C for 1-2h to obtain Sodium titanate nanowires or potassium titanate nanowires.

More preferably, the specific steps of S1 are: preparing a 10mol/L sodium hydroxide or potassium hydroxide solution for subsequent use;

Weigh the titanium sheet, add the titanium sheet and sodium hydroxide or potassium hydroxide solution into the hydrothermal reaction kettle in sequence according to the solid-to-liquid ratio of 1g: 15-25ml; keep warm at 140-160°C for 8-12 hours, then After cooling to room temperature, the titanium sheet is taken out, washed, centrifuged, dried, and calcined at 420-450° C. for 1-2 hours to obtain sodium titanate nanobelts or potassium titanate nanobelts.

More preferably, the specific steps of S1 are: respectively measure butyl titanate and ethanol according to the volume ratio of 1:3-5, and prepare 10 mol/L sodium hydroxide or potassium hydroxide solution for later use;

Slowly add butyl titanate to ethanol, then add 10 mol/L sodium hydroxide or potassium hydroxide solution equal to the volume of butyl titanate, mix well, let stand for 2 hours to form a sol, and add the sol to In a hydrothermal reaction kettle, keep warm at 180-200°C for 12 hours, then cool naturally to room temperature, wash, centrifuge and dry the reaction product, then calcinate at 440-460°C for 1-2 hours to obtain sodium titanate nanofibers or potassium titanate Nanofibers.

Preferably, in S1, the preparation process of the Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic vitrified bond powder is as follows;

According to the ratio of mass ratio 8:5:72:15, take sodium carbonate, aluminum hydroxide, silicon dioxide and boric acid respectively, and set aside;

After mixing the sodium carbonate, aluminum hydroxide, silicon dioxide and boric acid, ball mill to 200-400 mesh, press into a block, and melt the block at 1200-1300°C in a glass melting furnace, and the heating time is After 0.5-2 hours, the melt is water-quenched, and the product is dried and ball-milled to a particle size of less than 200 mesh to obtain the Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic vitrified powder.

Preferably, in S3, the acid salt one-dimensional nanomaterial is added to the Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic ceramic bond powder in an amount of 1-3%, Mix well and disperse uniformly to prepare nano vitrified bond.

The present invention also provides a nano-ceramic bond prepared by any of the methods described above.

Preferably, the nano-ceramic bond provided by the present invention is used in the preparation of ordinary ceramic abrasive tools or superhard abrasive tools.

The technical solution of the present invention has the following beneficial effects:

(1) Since the existing ordinary vitrified bond has low strength, high sintering temperature and its own brittleness, the present invention overcomes the common vitrified bond by adding a titanate one-dimensional nanomaterial to prepare the nano-ceramed bond Not only greatly reduces the sintering temperature of the bond, saves energy, but also significantly improves the strength of the vitrified bond, which can be well applied to ceramic abrasive tools.

(2) The sintering temperature of the nano-ceramic bond prepared by the present invention is low, and the strength is high, which can well meet the needs of ceramic abrasive tools in precision machining, and the prepared nano-ceramic bond has a good infiltration of abrasive materials, which is very large. To a certain extent, the holding force of superhard abrasives is improved, and the grinding effect is significantly improved.

detailed description

In order to enable those skilled in the art to better understand that the technical solutions of the present invention can be implemented, the present invention will be further described below in conjunction with specific examples, but the given examples are not intended to limit the present invention.

When the examples give numerical ranges, it should be understood that, unless otherwise stated in the present invention, the two endpoints of each numerical range and any value between the two endpoints can be selected. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition to the specific methods, equipment, and materials used in the embodiments, according to those skilled in the art's grasp of the prior art and the description of the present invention, the methods, equipment, and materials described in the embodiments of the present invention can also be used Any methods, apparatus and materials of the prior art similar or equivalent to the practice of the present invention.

A novel nano-ceramic bond of the present invention is specifically prepared by the following steps:

S1: Preparation of titanate one-dimensional nanomaterials;

S2: Provide Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic vitrified bond powder;

S3: Add the titanate one-dimensional nanomaterial prepared in S1 to the basic vitrified bond powder in an amount of 0.2-5 wt%, and fully mix and disperse evenly to obtain the nano vitrified bond.

It should be noted here that the raw materials used to prepare the above titanate one-dimensional nanomaterials are titanium dioxide, metallic titanium, titanium alloys or titanium salts. The above-mentioned titanate one-dimensional nanomaterials obtained are sodium titanate nanowires, potassium titanate nanowires, sodium titanate nanofibers, potassium titanate nanofibers, sodium titanate nanobelts, and potassium titanate nanobelts. any kind.

The technical solution of the present invention will be described with specific examples below.

Example 1

A novel nano-ceramic bond, the preparation process of which is as follows:

First prepare a 10mol/L sodium hydroxide solution, take 45mL of the sodium hydroxide solution, place it in a plastic beaker, and stir it magnetically to make the solution fully uniform; then weigh 1.5g of titanium dioxide powder, dissolve it in the above sodium hydroxide aqueous solution, and fully Stir until it becomes a homogeneous milky mixture solution. Add the mixed solution into the reaction kettle, keep it warm at 150°C for 10h, then cool it down to room temperature naturally, wash it thoroughly with deionized water, then centrifuge, wash with deionized water and absolute ethanol, centrifuge, dry, and place in a muffle furnace Calcined at 450°C for 2 hours to obtain sodium titanate nanowires.

According to the mass ratio of 8:5:72:15, weigh the raw materials sodium carbonate, aluminum hydroxide, silicon dioxide and boric acid respectively, mix the four raw materials, ball mill them to 300 mesh, and press them into a block. Use a glass melting furnace to melt at 1300°C, the heating time is 1h, and then quench the melt with water, and the product is dried, ball milled, and crushed with a particle size of less than 200 mesh to obtain Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ base vitrified bond powder. To the above Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic ceramic bond powder, add the above sodium titanate nanowires according to the addition amount of 3%, fully mix and disperse uniformly, and obtain a nano ceramic bond .

The performance test of the nano-ceramic bond prepared in Example 1 shows that the flexural strength reaches a maximum of 98MPa, the refractoriness is 700°C, the flexural strength is increased by 50%, and the sintering temperature is reduced by 135°C compared with no addition.

Example 2

A novel nano-ceramic bond, the preparation process of which is as follows:

First prepare 10mol/L sodium hydroxide solution, take 45mL of sodium hydroxide solution, put it in a plastic beaker, and stir it magnetically to make the solution fully uniform; then weigh 2.5g of titanium sheet and put it in a hydrothermal reaction kettle, and then Add the sodium oxide solution into the hydrothermal reaction kettle, keep it warm at 150°C for 12 hours, then cool it down to room temperature naturally, take out the titanium sheet and wash it with deionized water, then centrifuge, wash with deionized water and absolute ethanol, centrifuge and dry , and calcined at 450° C. for 2 h in a muffle furnace to obtain sodium titanate nanobelts.

According to the mass ratio of 8:5:72:15, weigh the raw materials sodium carbonate, aluminum hydroxide, silicon dioxide and boric acid respectively, mix the four raw materials, ball mill them to 300 mesh, and press them into a block. Use a glass melting furnace to heat at 1300°C for 1 hour, dry the heated product, ball mill it, and pulverize it to 200 mesh to obtain the basic vitrified bond of Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ powder.

Add the above-mentioned sodium titanate nanobelts to the above-mentioned Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic vitrified powder, according to the addition amount of 3%, fully mix and disperse uniformly, and obtain a nano-ceramic bond .

The performance test of the nano-ceramic bond prepared in Example 2 shows that the flexural strength reaches a maximum of 95MPa, and the refractoriness is 710°C.

Example 3

A novel nano-ceramic bond, the preparation process of which is as follows:

Measure 45mL of ethanol, pour it into a 100mL beaker, stir vigorously on a magnetic stirrer, slowly add 15mL of butyl titanate, after the solution is stable, continue to add 15mL of 10mol/L potassium hydroxide aqueous solution drop by drop under strong stirring, Continue to stir steadily for 20 minutes, then stand still for 2 hours without any abnormality, add the sol to the hydrothermal reaction kettle, keep it at 180°C for 12 hours, then cool it down to room temperature naturally, then fully wash with deionized water and absolute ethanol, centrifuge, and dry. And calcining at 450° C. for 2 hours in a muffle furnace to obtain potassium titanate nanofibers.

According to the mass ratio of 8:5:72:15, weigh the raw materials sodium carbonate, aluminum hydroxide, silicon dioxide and boric acid respectively, mix the four raw materials, ball mill them to 300 mesh, and press them into a block. Heating in a glass melting furnace at 1250°C for 1 hour, drying, ball milling and pulverizing the heated product to 200 mesh to obtain the basic vitrified bond of Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ powder.

Add the above-mentioned potassium titanate nanofibers to the above-mentioned Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic vitrified bond powder according to the addition amount of 1%, and mix well and disperse uniformly to obtain a nano-ceramic bond .

The performance test of the nano-ceramic bond prepared in Example 3 shows that the flexural strength reaches a maximum of 101MPa, the refractoriness is 705°C, the flexural strength is increased by 55% compared with that without addition, and the sintering temperature is reduced by 130°C.

Example 4

A novel nano-ceramic bond, the preparation process of which is as follows:

First prepare a 10mol/L sodium hydroxide solution, take 45mL of the sodium hydroxide solution, place it in a plastic beaker, and stir it magnetically to make the solution fully uniform; then weigh 2.0g of titanium dioxide powder, dissolve it in the above sodium hydroxide aqueous solution, and fully Stir until it becomes a homogeneous milky mixture solution. Add the mixed solution into the reaction kettle, keep it warm at 150°C for 6 hours, cool it down to room temperature naturally, wash it thoroughly with deionized water, then centrifuge, wash with deionized water and absolute ethanol, dry it, and put it in a muffle furnace Sodium titanate nanowires can be obtained by calcining at 430° C. for 1 hour.

According to the mass ratio of 8:5:72:15, weigh the raw materials sodium carbonate, aluminum hydroxide, silicon dioxide and boric acid respectively, mix the four raw materials, ball mill them to 400 mesh, and press them into blocks. Heating in a glass melting furnace at 1250°C for 1 hour, drying, ball milling and pulverizing the heated product to 200 mesh to obtain the basic vitrified bond of Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ powder.

To the above Na ₂ O-Al ₂ O ₃ -SiO ₂ -B ₂ O ₃ basic ceramic bond powder, add the above sodium titanate nanowires according to the addition amount of 3%, fully mix and disperse uniformly, and obtain a nano ceramic bond .

The performance test of the nano-ceramic bond prepared in Example 4 shows that the flexural strength reaches a maximum of 106MPa, the refractoriness is 685°C, the flexural strength is increased by 63% compared with that without addition, and the sintering temperature is reduced by 150°C.

The above-mentioned embodiments are only preferred embodiments for fully illustrating the present invention, and the scope of protection thereof is not limited thereto. The equivalent substitutions or transformations made by those skilled in the art on the basis of the present invention are all within the protection scope of the present invention, and the protection scope of the present invention shall be determined by the claims.

Claims (10)

1. a kind of preparation method of novel nano vitrified bond, it is characterised in that comprise the following steps：

S1：Prepare titanate one-dimensional nano material；

S2：Na is provided₂O-Al₂O₃-SiO₂-B₂O₃Basic vitrified bond powder；

S3：Titanate one-dimensional nano material prepared by S1 is added to basic vitrified bond powder by the addition of 0.2~5wt% In end, it is sufficiently mixed and is uniformly dispersed, nano-grade ceramic binding agent is obtained.

2. the preparation method of nano-grade ceramic binding agent according to claim 1, it is characterised in that prepare the titanate one Raw material used by dimension nano material is titanium dioxide, Titanium, titanium alloy or titanium salt.

3. the preparation method of nano-grade ceramic binding agent according to claim 1 and 2, it is characterised in that the titanate one Dimension nano material is sodium titanate nano wire, Nano lines of potassium titanate, sodium titanate nanofiber, potassium titanate nanofiber, sodium titanate are received Rice band, any one in potassium titanate nanobelt.

4. the preparation method of novel nano vitrified bond according to claim 3, it is characterised in that the specific steps of S1 For：

The NaOH or potassium hydroxide solution of 10mol/L are prepared, it is standby；

Titania powder is weighed, according to solid-to-liquid ratio 1g：The ratio of 20~40ml, NaOH is added to by titania powder Or in potassium hydroxide solution, fully dissolving obtains mixed solution；

The mixed solution is added in hydrothermal reaction kettle, 8~10h is incubated at 140~160 DEG C, then naturally cooled to Room temperature, after scrubbed, centrifugation, drying, calcines 1~2h at 420~450 DEG C, obtains sodium titanate nano wire or potassium titanate nanometer Line.

5. the preparation method of novel nano vitrified bond according to claim 3, it is characterised in that the specific steps of S1 For：

The NaOH or potassium hydroxide solution of 10mol/L are prepared, it is standby；

Titanium sheet is weighed, according to solid-to-liquid ratio 1g：The ratio of 15~25ml, titanium sheet and NaOH or potassium hydroxide solution are added successively In entering hydrothermal reaction kettle；8~12h is incubated at 140~160 DEG C, room temperature is then naturally cooled to, take out titanium sheet and it is scrubbed, After centrifugation, drying, 1~2h is calcined at 420~450 DEG C, obtain sodium titanate nanobelt or potassium titanate nanobelt.

6. the preparation method of novel nano vitrified bond according to claim 3, it is characterised in that the specific steps of S1 For：

According to volume ratio 1：3~5 ratio measures butyl titanate and ethanol respectively, and prepares the NaOH or hydrogen of 10mol/L Potassium oxide solution, it is standby；

Butyl titanate is slowly added into ethanol, the NaOH or hydrogen of the 10mol/L isometric with butyl titanate is added Potassium oxide solution, after being sufficiently mixed, stands 2h and forms colloidal sol, the colloidal sol is added in hydrothermal reaction kettle, 180~200 DEG C Insulation 12h, then naturally cools to room temperature, product is scrubbed, centrifugation, dry after, calcine 1 at 440~460 DEG C~ 2h, obtains sodium titanate nanofiber or potassium titanate nanofiber.

7. the preparation method of novel nano vitrified bond according to claim 1, it is characterised in that described in S1 Na₂O-Al₂O₃-SiO₂-B₂O₃The preparation process of basic vitrified bond powder is；

According to mass ratio 8:5:72:15 ratio, weighs sodium carbonate, aluminium hydroxide, silica and boric acid respectively, standby；

After the sodium carbonate, aluminium hydroxide, silica and boric acid are mixed, 200~400 mesh are milled to, are pressed into block, will The block is melted with glass melting stove at 1200~1300 DEG C, and the heat time is 0.5~2h, and melt then is entered into water-filling Quench, product is less than 200 mesh, obtains the Na through drying, ball milling, grinding particle size₂O-Al₂O₃-SiO₂-B₂O₃Basic vitrified bond Powder.

8. the preparation method of novel nano vitrified bond according to claim 1, it is characterised in that in S3, to described Na₂O-Al₂O₃-SiO₂-B₂O₃In basic vitrified bond powder, the hydrochlorate 1-dimention nano is added according to 1~3% addition Material, is sufficiently mixed and is uniformly dispersed, and nano-grade ceramic binding agent is obtained.

9. a kind of nano-grade ceramic binding agent, it is characterised in that the method as described in any one of claim 1~8 is prepared.

10. nano-grade ceramic binding agent according to claim 9, it is characterised in that in conventional ceramic grinding tool or super-hard abrasive tool Application in preparation.